反应详情

3-Hydroxy-5-methylsulfonylbenzoic acid (D13) was dissolved in DMF (42 ml) and treated with caesium carbonate (14.1 g) and methyl iodide (8.6 ml) The mixture was sonicated under argon for 45 min. and stirred for 3 h at room temperature. The DMF was evaporated in vacuo and the residue was partitioned between ethyl acetate and 2M hydrochloric acid. The aqueous layer was re-extracted twice with ethyl acetate and the combined extracts were washed with sodium bicarbonate solution, sodium thiosulfate solution, water and brine, dried (Mg SO4) and evaporated to a semi solid. Trituration with ether gave D14 (2 crops, 2.94 g).

1. customwas sonicated under argon for 45 min.
2. customThe DMF was evaporated in vacuo
3. customthe residue was partitioned between ethyl acetate and 2M hydrochloric acid
4. extractionThe aqueous layer was re-extracted twice with ethyl acetate
5. washthe combined extracts were washed with sodium bicarbonate solution, sodium thiosulfate solution, water and brine
6. dry with materialdried (Mg SO4)
7. customevaporated to a semi solid
8. customTrituration with ether gave D14 (2 crops, 2.94 g)